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Naji, M. |
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Motta, Antonella |
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Aletan, Dirar |
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Mohamed, Tarek |
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Ertürk, Emre |
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Taccardi, Nicola |
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Petrov, R. H. | Madrid |
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Alshaaer, Mazen | Brussels |
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Bih, L. |
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Casati, R. |
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Kočí, Jan | Prague |
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Kalteremidou, Kalliopi-Artemi | Brussels |
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Azam, Siraj |
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Ospanova, Alyiya |
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Blanpain, Bart |
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Ali, M. A. |
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Popa, V. |
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Rančić, M. |
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Ollier, Nadège |
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Azevedo, Nuno Monteiro |
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Landes, Michael |
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Rignanese, Gian-Marco |
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Oliver, Allen G.
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article
Co-crystallization of dimethyl <i>N</i>-cyanodithioiminocarbonate and bis[(aqua)-<i>µ</i> <sub>2</sub>-hydroxy-<i>n</i>-butyldichlorotin(IV)]
Abstract
<jats:title>Abstract</jats:title><jats:p>The one-pot reaction of dimethyl <jats:italic>N</jats:italic>-cyanodithioiminocarbonate, [(MeS)<jats:sub>2</jats:sub>C=N–C≡N] with <jats:italic>n</jats:italic>-butyltin trichloride, Sn(<jats:italic>n</jats:italic>-Bu)Cl<jats:sub>3</jats:sub> led to a dinuclear complex [Sn(<jats:italic>n</jats:italic>-Bu)Cl<jats:sub>2</jats:sub>(OH)(H<jats:sub>2</jats:sub>O)]<jats:sub>2</jats:sub> which co-crystallized with two [(MeS)<jats:sub>2</jats:sub>C=N–C≡N] molecules (<jats:bold>1</jats:bold>). The product was investigated by single-crystal X-ray diffraction analysis. Compound <jats:bold>1</jats:bold> crystallizes in the triclinic space group <jats:inline-formula id="j_znb-2022-0061_ineq_001"><jats:alternatives><m:math xmlns:m="http://www.w3.org/1998/Math/MathML" overflow="scroll"><m:mrow><m:mi>P</m:mi><m:mover accent="true"><m:mn>1</m:mn><m:mo>‾</m:mo></m:mover></m:mrow></m:math><jats:tex-math>$P{1}$</jats:tex-math><jats:inline-graphic xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="graphic/j_znb-2022-0061_ineq_001.png" /></jats:alternatives></jats:inline-formula> with <jats:italic>a</jats:italic> = 6.8048(6), <jats:italic>b</jats:italic> = 11.0645(9), <jats:italic>c</jats:italic> = 12.4240(10) Å, <jats:italic>α</jats:italic> = 66.3120(10), <jats:italic>β</jats:italic> = 75.6070(10), <jats:italic>γ</jats:italic> = 72.2940(10)°, <jats:italic>V</jats:italic> = 807.42(12) Å<jats:sup>3</jats:sup>, <jats:italic>Z</jats:italic> = 1 and <jats:italic>Z</jats:italic>′ = 0.5. In the complex, two aqua-<jats:italic>n</jats:italic>-butyltin dichloride, [Sn(<jats:italic>n</jats:italic>-Bu)Cl<jats:sub>2</jats:sub>(H<jats:sub>2</jats:sub>O)]<jats:sup>+</jats:sup>, moieties are bridged by two hydroxide OH<jats:sup>−</jats:sup> ions. Two inner O2–H2OB⋯Cl2 hydrogen bonds strengthen the dinuclear component which is connected to its neighbours through a O1–H1O⋯Cl1 hydrogen bond pattern giving rise to a network of infinite chains running parallel to the (100) direction. The dimethyl <jats:italic>N</jats:italic>-cyanodithioiminocarbonate molecules are linked to these infinite chains through O2–H2OA⋯N1 hydrogen bonding interactions of D type. The [(MeS)<jats:sub>2</jats:sub>C=N–CN] molecules exhibits a minor positional disorder. These hydrogen bonding interactions lead to cyclic patterns generating <jats:inline-formula id="j_znb-2022-0061_ineq_002"><jats:alternatives><m:math xmlns:m="http://www.w3.org/1998/Math/MathML" overflow="scroll"><m:mrow><m:msubsup><m:mtext>R</m:mtext><m:mn>1</m:mn><m:mn>1</m:mn></m:msubsup><m:mrow><m:mo>(</m:mo><m:mn>6</m:mn><m:mo>)</m:mo></m:mrow></m:mrow></m:math><jats:tex-math>${{R}}_{1}^{1}(6)$</jats:tex-math><jats:inline-graphic xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="graphic/j_znb-2022-0061_ineq_002.png" /></jats:alternatives></jats:inline-formula> and <jats:inline-formula id="j_znb-2022-0061_ineq_003"><jats:alternatives><m:math xmlns:m="http://www.w3.org/1998/Math/MathML" overflow="scroll"><m:mrow><m:msubsup><m:mtext>R</m:mtext><m:mn>2</m:mn><m:mn>2</m:mn></m:msubsup><m:mrow><m:mo>(</m:mo><m:mn>8</m:mn><m:mo>)</m:mo></m:mrow></m:mrow></m:math><jats:tex-math>${{R}}_{2}^{2}(8)$</jats:tex-math><jats:inline-graphic xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="graphic/j_znb-2022-0061_ineq_003.png" /></jats:alternatives></jats:inline-formula> rings. Weak C–H⋯Cl hydrogen bonds also contribute to the stability of the crystal structure.</jats:p>